|
the
Hive BB ![]() Methods
Discourse ![]() Hash
making question
|
| next newest topic | next oldest topic |
| Author | Topic: Hash making question |
| Dope
Amine Hive Bee |
I'm interested in making and isomerising hash oil from some extra leaf layin' around. Hypothetically, I'm using acetone cuz it is supposed to be superior to alcohol for solubility of THC. I know that with alcohol, when you want to separate polar from non-polar, you add water to the alcohol so that it becomes insoluble in your non-polar solvent. My question is can you treat acetone the same as if it was alcohol and add water to acetone to make it insoluble in DCM? Otherwise what would be a good way to separate the oil from the polar stuff (sulfuric acid and chloriphyl)? |
| Rhodium Pimp Master |
You need to add lots of water to make an acetone layer "insoluble" in DCM... Check out the book "Marijuana Chemistry" by M. Starks available from http://www.promind.com/ |
| Dope
Amine Hive Bee |
Could anyone tell me if it is really worth doing the separation. I'm thinking that one could use HCl instead of sulfuric and then it would just evaporate off with the acetone. |
| Rhodium Pimp Master |
I don't believe you can do the acid reflux in acetone, it will probably react with the THC in that environment. Use ether/alcohol/DCM or something like that. HCl can be used, but if you use aqueous HCl you cannot use DCM as solvent, as it is too non-polar. |
| Dope
Amine Hive Bee |
Too late.
Already did it with acetone and about the same ammount of H+ ions from HCl
that one would get from the recommended ammount of sulfuric acid in the
literature. Bummer. I'm confused, are you saying that like DCM, acetone is
too non-polar and so there will be no reaction, or are you saying that HCl
in acetone is an inviornment that will ruin my oils.
|
| drunkenmaster Hive Bee |
99% ipa is all you should ever use with weed oil, H2SO4 reflux, and a bone activated charcoal filter somewhere in there, and it is possible to yield totally colorless oil. stay tuned and i will post a complete procedure here soon. |
| drunkenmaster Hive Bee |
not ipa ethyl-methyl my mistake. Reply from The Dislexicchemist: One day when I was a minor 14 years old (teehee) I Dreamt thusly: I Took a large amount of shake and soaked it in pet ether ( IPA works to) for 1/2 hours for porsonal or 12 to 24 hrs for commmercial grade oil, then filter. The the pet ether was distilled off to crude oil, this oil was dissolved in either IPA or MeOH, (If you use IPA in the begining soak you don't have to distill it down for this step) Take the oil alcohol mix and add H2O and pet ether shake and let sit shake more then sep the pet ether off, take the pet ether oil mix and distill down to oil. Now take the oil and mix it with MeOH, 1g of oil to 10 ml of alcohol, stir in 1 drop of 90% H2S04, the oil. MeOH H2SO4 Mix is then refluxed for 4-6 h. The refluxed mix was then mixed with H2O and pet ether, 5% baking soda H2O mix was added and the flask was then stoppered and inverted, pressure being realeased periodically. this was inverted (mixed) 25x then sepped. this was reapeated until the Ph of the H2O was base. then it was washed with pure H2O and then separate the pet ether. the pet ether is distilled down to yield a very light red oil which was translucent. This oil was dissolved in IPA, and bone activated charcoal was added. this was filtered to remove charcoal, and filtered again through silicate sand. the IPA was distilled to yield a tolally colourless oil. There is a way to take this oil and react it with acetic anyhydride but i'll leave it to you since it is not the safest thing to to. btw: N2 atmosphere would make it safer. let's hear it for our guest speaker dislexicchemist! high times sucks, dm |
| AbSoLuTe Hive Bee |
Extract with Pet ether, using a Soxhlet extraction setup, remove pet ether, dissolve in Ethanol react/reflux each gram with a drop of H2So4(conc), boil 12 hours, add 50mg/5 grams oil activated charcoal,filter evap Ethanol slowly, lovely amber oil that is good for any purpose. I have done this as per the instruction from "CANNABIS ALCHEMY, The Art Of Modern Hashmaking" by Gold I think. Tells you how to take it all the way to a pure white powder pure THC, but I believe that there are better White powders out there. |
| Osmium PimpBee |
THC will always be an oil, not a white powder. Butane is the solution for your extraction questions bees.
Butane... |
| Sumerian Hive Bee |
Post isomerization mix should be extracted with ether,not initial extraction to obtain crude oil.Ether is very selective,if this is used in the initial extraction one will get only a small amount of available oil for isomerization.Isomerizing's whole purpose is conversion to higher rotating THC's.Alcohol extraction first will get all available THC's,then Isomerize with 1drop of sulphuric acid per 10 grams of alcohol(99%IPA used to dissolve oil) reflux 3-4hrs.Neutralize post mix with 5%baking soda/H2O,til acid is gone.Then extract this alcohol/oil mix with ether or toluene,evap solvent,will leave nice golden oil that has increased potentcy.Get some acetic anhydride and make the acetate,2x more potent,255 gain in weight. Osmium;crystalline THC is possible,but is a long process involving,fractional distillation,chromo,then a parr bomb,and so on.I have tried some product a few years back that was made by a mad scientist using this route,2 lines was like a mini-acid trip with out the visuals.
|
| Sumerian Hive Bee |
Change one thing in the above post; Flood post iso alc/oil/acid mix with H2O and extract with non-polar(ether or toluene) then wash this with the 5%soda/H2O mix.Evap solvent voila isomerized hash oil.Or one could strain solvent/oil mix through activated charcoal then evap solvent.This will lighten up color considerably. Btw Osmium;THC can be made crystalline,but it is a lengthy process involving gas chromo,fractional dist,parr bomb,and so on.Pretty interesting process.Sumerian once new a mad scientist that presented a small pile of white powder for his inhaling pleasure,it was crystallized THC,very interesting buzz,almost acid-like without the visuals.Lasted for 8 hours
|
| Sumerian Hive Bee |
Sorry about the repitition in my above posts,too much oil this morning ![]() Also THC acetate gains 25% in weight not 255,my typing is a lttle chaotic today. |
| Methyl
Man Hive Bee |
This is something I threw together a while back. It's here on the Hive in a post in fact, but what the hell, here it is again anyway: ====================== For those of us who never quite got over the loss when fine-quality hash oil disappeared from the market, and for all cannabis connoisseurs everywhere, it would be my honor to write up what is in my opinion the easiest, highest-yielding and most selective cannabis oil extraction method available to date. Others have posted about this method before me; I simply want to write it up in a little more detail than has been provided to this point. In my mind, the credit for being the first to introduce this method to bees on the Lycaeum goes to Freejon. A big thanks goes out to gyrogearloose also for perpetuating it here lately. This method uses perfectly OTC butane gas (use the lighter refiller type, not the camping supply type which has a nasty odorizer in it) as the extraction solvent, and requires nothing even remotely suspicious or difficult to purchase. (I have heard that CO2 works also, but I haven't tried that yet. Obviously it's a safer choice, so it would be a good thing to move up to once butane has been tried a time or two.) The only other thing needed is about $2.00 worth of PVC pipe: a section 1.5 (one and a half) feet long and 1 & 3/4" diameter (outer diameter I believe), and two end caps. Threads are not necessary. For reasons not yet clear to those of us investigating these things "unofficially," butane and CO2 (and perhaps other gases with similar low-boiling properties) selectively solvate the desireable fraction(s) of cannabis oils, pulling out only a beautiful amber "honey oil" and leaving the undesireable vegetative oils, waxes, chlorophyll, etc. behind in the plant matter. Even unsmokable shade leaves produce a wonderfully clean and potent oil. I have every reason to suspect that this would work splendidly to extract a super-strong and tasty oil from gross, unpalatable "schwag" commercial pot,and of course, the better grade of weed you put it in, the better the resulting oil. METHOD: 1) In one of the end caps, drill a single small hole in the center.
This hole should be correctly sized to receive the little outlet nozzle of
your butane can. The butane moves down the pipe, extracting the cannabis as it goes. When it gets to the bottom (~30 seconds after dispensing), it begins to drain into the receiving vessel. Notice the pale, glowing yellow-green-gold hue of the extract. It is obvious no chlorophyll was pulled out of the herb. Over approximately five to eight minutes, the butane extract will finish draining from the pipe to the receiving vessel. Maintain caution with the pipe, however, since there is a lot of residual butane still evaporating from within the pipe (notice the stream of fumes coming from the top hole). When it slows down to a drop every few seconds, you can tap on the top hole with your finger and it will help push the last of the liquid butane out (or one can gently blow into the hole to do the same thing. Remember, NO SMOKING!!). Being very low-boiling and volatile, the collected butane will likely begin boiling at ambient temperature. The receiving vessel will gradually frost up as the butane cools it down, slowing down its rate of evaporation, but you can speed this up again simply by holding it in your hands. A better way is to set it in a saucepan containing a little bit of warm water. Watch the butane start bubbling madly with the increase in temperature and marvel at its low boiling point. Again, be doing this outdoors with a nice breeze! When the majority of the butane is gone, but before the oil is starting to thicken, you have the choice of putting the oil into a vial or leaving it in your receiving vessel. If you choose to put it into a vial, it's important that you use an oversized one, i.e. one that can hold several times the volume of your solution. (I learned the hard way about this, thanks to the volatile temperament of butane. I had filled a vial almost all the way to the top and was preparing to drop those last couple drops in so that cleverly, I could let the last of the butane evaporate from the vial and the oil would all be neatly contained. But when the last drops hit the mother lode in the vial, they changed its temperature upward by a hair and it all "superboiled" out of the vial and onto my fingers, which of course startled me and caused me to drop the vial. So heed me when I say to use an oversize vial. Now I just leave it in a 140 mL beaker for safety's sake.) It's a trip to watch the last traces of butane make sticky bubbles in the beautiful mess of amber residue as you apply that last bit of gentle heat. The final product is a deep yellow-amber oil of the highest quality, incredibly pure and potent. I remember well some of the prime "honey oil" hash oils that hit the market in the late 1970s, and this stuff stands up to any of them. It's amazing how this method extracts only the good fraction and leaves the junk in the weed. But that's exactly what it does. Note also that this oil has a somewhat higher melt/vaporization point than traditional hash oils; the traditional dispensing method (dipping a needle or paper clip in, getting some goop on the end, and warming it with a flame to get it to drip off into your bowl) still works with this stuff, but it seems you have to be more careful with it because it doesn't heat to liquid state as quickly or in the same manner, and it can more easily be allowed to burn up on your needle. So be careful. Those who prefer a tincture-like preparation can of course thin the product a little with a bit of warm high-percentage alcohol like Everclear or 90-whatever-% isopropyl, then drop it onto buds or let a joint absorb some, then let the alcohol evaporate. I also observed that unlike hash oil derived from traditional methods, this product is not readily soluble in room-temp alcohol; it needed to be warmed before it dissolved fully. So there it is. Spread the word far and wide: hash oil is
BACK! One note I would add though is that it seems to be unknown by everyone
whether butane will leach any nasties out of PVC (I never could find any
solubility info regarding that pair), so if possible it would be better to
use steel pipe. If you don't drill the holes yourself though I would still
use a PVC cap for the top piece so that they don't think you're making a
pipe bomb. |
| Starlite Hive Bee |
You da MAN methyl!!! |
| Sumerian Hive Bee |
Its a homegrown super critical fluid extractor,gotta love it!!!!!! I've often contemplated building a pvc type device and pass CO2 through it.I know what I'm doing tomorrow
|
| pHas3d PimpBee |
Now I love all this "super critical" hooblah, but riddle me this... Why the hell doesnt propane work? Seems to this glue huffer to be a thc solvent and better in the super critical department. Not to mention, you can find lots of propane. Big things of butane are non existant in my neck of the woods. BTW, propane deffinatly doesnt work but it is cool
to watch it boil away after you wasted a bunch of time.pHas3d |
| Osmium PimpBee |
I'm not sure, but I guess the temp will be too low with propane, slowing down the THC dissolution too much. Butane is easily liquified, most of the propane will probably leave the pipe still in a gaseous state. |
| zephler NewBee |
After making oil and hash for a couple of years, I have come up with what is probably the healthiest method....Steam Distillation, it takes a bit of glassware but its definitely worth it man. Using all those chems, no matter what you are gonna have residual crap laying around in the oil, making a natural product, horribly contaminated with junk. Steam distillation uses water! Way better for you and your customers. Your body will thank you, after all don't you feel kind of guilty smoking smothing that has been treated with non polar solvents?
quote: |
| pHas3d PimpBee |
Well, this bee just might have every damm piece of glass in the world, but still doesnt know how steam distilatin works. I dig soxlet, and normal extractions of all kind, but how does one rig apperatus for doing that. Step by step for retards like myself would be appreciated. pHas3d |
| pHas3d PimpBee |
That was a bit tough to figure out. I would like to know how one would rig glassware to steam distill. pHas3d |
| KrZ Hive Bee |
Phased: The super critical shit got me too. I think HULLABALLO would be the best term to describe that, and a number of other items... Anyways, the only thing I've ever bothered with was makeing hash-oil out of some leaves, just dumped it in some EtOH in the blender zaped it, and refluxed the mess for a couple of hours, distilling off the alcohol gave a thick oil which was plenty potent for my needs. But who knows, maybe this isomerized stuff is really the shiz-nit-o-bam snip-snap-sally, anyone seen god or been abducted by aliens on it? |
| Starlite Hive Bee |
re: Steam Distillation... Saw one post here that had it down.. get a 20 lb pressure cooker ( or a flask with an addition funnel ) and use that as the steam source. Run a line into a glass tube pushed through a stopper into your 1 or 2 liter flask. Make sure the glass tube is pulled to a point. Now, load flask/p.c. with H20 and generate steam. Put your stuff in the 2nd flask/pot and add heat, while you add steam. The steam forms an azeotrope (10$ word meaning mixture) that causes the oil to evaporate at a much lower temperature and also busts up the cell structure ( should be ground anyway). The 2nd neck of the flask goes to a distillation arm to the condensor...all the goodies follow the steam into the condensor...then you have product!
|
| Sumerian Hive Bee |
Zeph: Steam distillation sounds nice,but it carries unwanted H20 soluables over with it.H20 soluables are inactive,so your oil's potential is cut drastically by introducing H20 into the equation. I have been making hash oil for 11 years and not once has any ill effects been felt by anyone.My secret,boiling out the solvent,it does evaporate you know. Try high temp. fractional vac. distillation of isomerized oil,that gives a far superior product. |
| Ageless
Trout Hive Bee |
I have a dean stark soxlet, is this what you use when you mention a soxlet extraction or could someone stear me in the proper direction. THX in advance Ageless Trout ------------------ |
| Dope
Amine Hive Bee |
Sumerian: Is your product as clean as the one discussed using supercritical fluid extraction? I know of someone who used acetone as the original solvent, refluxed with HCl, evaporated, disolved in IPA and added equal ammt. of h2o, extracted with DCM, and evaporated. Even after doing the DCM/H2O separation, the product oil was still blackish green. |
| Sumerian Hive Bee |
In my cannabis endeavors the initial extraction of oil with 99%IPA is black/green in color prior to isomerization.The post isomerization has a dark golden hue to it.The green is gone so to speak,and replaced with the dark golden brown hue. After extraction with non-polar solvent and neutralization,this tends be a light golden color.If this is re-dissolved in 99%IPA and passed through some activated charcoal,it will lighten up even more.The only time I get a clear/clear oil,is when I distill it under a vac. Its a long route to get it,but its fun chemistry.If you do manage to make the clear oil,turn on a few friends and you'll become an instant ganja god
|
| Sumerian Hive Bee |
One last thing; IMO I think that Hcl acid is the wrong choice for isomerizing.Sulfuric acid is the one you want.Also replace the acetone with 99%IPA or denatured alcohol.I'm not sure of how much of an indicator the color is,but the blackish green you describe sounds like no isomerization took place.For a good isomerization the conditions should be vigorous,and I think that is what is lacking with the acetone/Hcl mix,not enough vigor.DCM is a bottom feeder,try a top feeder like toluene or ether next time.You'll get a cleaner extract. |
|
All times are CT (US) |
next newest topic | next oldest topic |
|
|
Powered by: Ultimate Bulletin Board, Version 5.43c
© Infopop Corporation
(formerly Madrona Park, Inc.), 1998 -
2000.